# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Yamada, Hiroko'
_publ_contact_author_email       yamada@chem.sci.ehime-u.ac.jp

_publ_section_title              
;
New synthesis of meso-free-[14]triphyrin(2.1.1)
by McMurry coupling and its derivatization to Mn(I) and Re(I) complexes
;
loop_
_publ_author_name
H.Yamada
D.Kuzuhara
Z.Xue
S.Mori
T.Okujima
Z.Shen
H.Uno

# Attachment '- MeBuEtTriphyrine.cif'

data__20100528_2
_database_code_depnum_ccdc_archive 'CCDC 790488'
#TrackingRef '- MeBuEtTriphyrine.cif'

#==============================================================================

# CHEMICAL DATA

_chemical_formula_sum            'C30 H39 N3 '
_chemical_formula_moiety         'C30 H39 N3 '
_chemical_formula_weight         441.66
_chemical_melting_point          ?

#==============================================================================

# CRYSTAL DATA
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.5650(3)
_cell_length_b                   6.28328(13)
_cell_length_c                   28.6812(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.3790(10)
_cell_angle_gamma                90.00
_cell_volume                     2530.81(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14653
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      68.2

#------------------------------------------------------------------------------

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_T_max  0.980
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'VariMax 2.4 kW Ultra fine focus'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 10.00
_diffrn_reflns_number            27028
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         68.21
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        68.21
_diffrn_measured_fraction_theta_full 0.998

#==============================================================================

_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_solution    SIR2004
_computing_structure_refinement  SHELXL97
_computing_publication_material  'CrystalStructure 3.8.2'
_computing_molecular_graphics    ?

#==============================================================================

_reflns_number_total             4635
_reflns_number_gt                3297
_reflns_threshold_expression     >2sigma(I)
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00073(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4635
_refine_ls_number_parameters     306
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1487
_refine_ls_wR_factor_gt          0.1343
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.045

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.86963(10) 0.5468(2) 0.28872(5) 0.0317(4) Uani 1 1 d . . .
H1 H 0.8338 0.5044 0.2605 0.038 Uiso 0.58(3) 1 calc PR . .
N2 N 0.73215(11) 0.3013(2) 0.25603(5) 0.0358(4) Uani 1 1 d . . .
N3 N 0.78104(10) 0.5515(2) 0.19912(5) 0.0331(4) Uani 1 1 d . . .
H3 H 0.8019 0.5070 0.2292 0.040 Uiso 0.42(3) 1 calc PR . .
C1 C 0.92580(12) 0.7214(3) 0.29584(6) 0.0313(4) Uani 1 1 d . . .
C2 C 0.97466(12) 0.7346(3) 0.34721(6) 0.0331(4) Uani 1 1 d . . .
C3 C 0.94418(13) 0.5640(3) 0.36912(6) 0.0331(4) Uani 1 1 d . . .
C4 C 0.87640(13) 0.4458(3) 0.33154(6) 0.0316(4) Uani 1 1 d . . .
C5 C 0.82326(13) 0.2640(3) 0.33582(6) 0.0336(4) Uani 1 1 d . . .
H5 H 0.8349 0.1948 0.3663 0.040 Uiso 1 1 calc R . .
C6 C 0.75323(13) 0.1811(3) 0.29629(6) 0.0323(4) Uani 1 1 d . . .
C7 C 0.70191(12) -0.0232(3) 0.28662(6) 0.0317(4) Uani 1 1 d . . .
C8 C 0.65519(12) -0.0212(3) 0.23847(6) 0.0319(4) Uani 1 1 d . . .
C9 C 0.67852(13) 0.1851(3) 0.21952(7) 0.0335(4) Uani 1 1 d . . .
C10 C 0.66444(13) 0.2695(3) 0.17274(6) 0.0333(4) Uani 1 1 d . . .
H10 H 0.6212 0.2008 0.1464 0.040 Uiso 1 1 calc R . .
C11 C 0.71270(13) 0.4529(3) 0.16391(6) 0.0320(4) Uani 1 1 d . . .
C12 C 0.70112(13) 0.5732(3) 0.11908(6) 0.0322(4) Uani 1 1 d . . .
C13 C 0.76152(13) 0.7447(3) 0.12959(6) 0.0332(4) Uani 1 1 d . . .
C14 C 0.81190(13) 0.7277(3) 0.18091(6) 0.0329(4) Uani 1 1 d . . .
C15 C 0.88168(13) 0.8661(3) 0.20920(7) 0.0351(4) Uani 1 1 d . . .
H15 H 0.8985 0.9813 0.1917 0.042 Uiso 1 1 calc R . .
C16 C 0.93002(13) 0.8630(3) 0.25818(7) 0.0347(4) Uani 1 1 d . . .
H16 H 0.9738 0.9769 0.2680 0.042 Uiso 1 1 calc R . .
C17 C 1.04536(13) 0.9026(3) 0.36954(7) 0.0398(5) Uani 1 1 d . . .
H17A H 1.0664 0.8809 0.4046 0.060 Uiso 1 1 calc R . .
H17B H 1.0157 1.0432 0.3626 0.060 Uiso 1 1 calc R . .
H17C H 1.1004 0.8939 0.3560 0.060 Uiso 1 1 calc R . .
C18 C 0.96778(13) 0.5068(3) 0.42178(6) 0.0367(5) Uani 1 1 d . . .
H18A H 1.0305 0.5686 0.4383 0.044 Uiso 1 1 calc R . .
H18B H 0.9732 0.3502 0.4250 0.044 Uiso 1 1 calc R . .
C19 C 0.89355(14) 0.5854(3) 0.44715(7) 0.0391(5) Uani 1 1 d . . .
H19A H 0.8293 0.5437 0.4276 0.047 Uiso 1 1 calc R . .
H19B H 0.9049 0.5141 0.4789 0.047 Uiso 1 1 calc R . .
C20 C 0.89570(15) 0.8249(3) 0.45476(7) 0.0458(5) Uani 1 1 d . . .
H20A H 0.8807 0.8959 0.4228 0.055 Uiso 1 1 calc R . .
H20B H 0.9610 0.8674 0.4726 0.055 Uiso 1 1 calc R . .
C21 C 0.82622(17) 0.9038(4) 0.48241(8) 0.0581(6) Uani 1 1 d . . .
H21A H 0.7612 0.8635 0.4649 0.087 Uiso 1 1 calc R . .
H21B H 0.8306 1.0590 0.4854 0.087 Uiso 1 1 calc R . .
H21C H 0.8422 0.8394 0.5147 0.087 Uiso 1 1 calc R . .
C22 C 0.70301(13) -0.1917(3) 0.32345(7) 0.0346(4) Uani 1 1 d . . .
H22A H 0.7692 -0.2124 0.3433 0.042 Uiso 1 1 calc R . .
H22B H 0.6811 -0.3275 0.3067 0.042 Uiso 1 1 calc R . .
C23 C 0.64009(15) -0.1376(3) 0.35666(7) 0.0441(5) Uani 1 1 d . . .
H23A H 0.6622 -0.0048 0.3739 0.066 Uiso 1 1 calc R . .
H23B H 0.6436 -0.2529 0.3801 0.066 Uiso 1 1 calc R . .
H23C H 0.5741 -0.1204 0.3373 0.066 Uiso 1 1 calc R . .
C24 C 0.58958(12) -0.1855(3) 0.20989(7) 0.0341(4) Uani 1 1 d . . .
H24A H 0.6041 -0.3255 0.2260 0.041 Uiso 1 1 calc R . .
H24B H 0.6002 -0.1969 0.1773 0.041 Uiso 1 1 calc R . .
C25 C 0.48579(14) -0.1297(3) 0.20509(8) 0.0458(5) Uani 1 1 d . . .
H25A H 0.4745 -0.1249 0.2373 0.069 Uiso 1 1 calc R . .
H25B H 0.4446 -0.2379 0.1854 0.069 Uiso 1 1 calc R . .
H25C H 0.4714 0.0096 0.1895 0.069 Uiso 1 1 calc R . .
C26 C 0.63246(13) 0.5121(3) 0.07198(6) 0.0373(5) Uani 1 1 d . . .
H26A H 0.6344 0.3557 0.0682 0.045 Uiso 1 1 calc R . .
H26B H 0.6536 0.5777 0.0452 0.045 Uiso 1 1 calc R . .
C27 C 0.52882(13) 0.5801(3) 0.06768(7) 0.0398(5) Uani 1 1 d . . .
H27A H 0.4860 0.5016 0.0405 0.048 Uiso 1 1 calc R . .
H27B H 0.5119 0.5395 0.0977 0.048 Uiso 1 1 calc R . .
C28 C 0.51207(14) 0.8167(3) 0.05934(7) 0.0463(5) Uani 1 1 d . . .
H28A H 0.5302 0.8579 0.0297 0.056 Uiso 1 1 calc R . .
H28B H 0.5540 0.8952 0.0868 0.056 Uiso 1 1 calc R . .
C29 C 0.40932(16) 0.8830(4) 0.05416(8) 0.0580(6) Uani 1 1 d . . .
H29A H 0.3671 0.8024 0.0278 0.087 Uiso 1 1 calc R . .
H29B H 0.4023 1.0356 0.0469 0.087 Uiso 1 1 calc R . .
H29C H 0.3924 0.8538 0.0844 0.087 Uiso 1 1 calc R . .
C30 C 0.77771(14) 0.9169(3) 0.09661(7) 0.0400(5) Uani 1 1 d . . .
H30A H 0.7377 0.8910 0.0638 0.060 Uiso 1 1 calc R . .
H30B H 0.8448 0.9176 0.0963 0.060 Uiso 1 1 calc R . .
H30C H 0.7612 1.0549 0.1081 0.060 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0320(9) 0.0279(9) 0.0360(8) -0.0010(6) 0.0104(7) -0.0013(7)
N2 0.0380(9) 0.0304(9) 0.0385(9) 0.0004(7) 0.0093(7) -0.0033(7)
N3 0.0339(9) 0.0299(9) 0.0374(9) 0.0006(7) 0.0129(7) -0.0004(7)
C1 0.0285(10) 0.0281(10) 0.0390(10) -0.0013(8) 0.0119(8) -0.0009(8)
C2 0.0295(10) 0.0300(11) 0.0418(10) -0.0020(8) 0.0129(8) 0.0007(8)
C3 0.0295(10) 0.0324(11) 0.0385(10) 0.0007(8) 0.0111(8) 0.0027(8)
C4 0.0315(10) 0.0274(10) 0.0368(10) -0.0011(8) 0.0108(8) 0.0014(8)
C5 0.0362(11) 0.0304(11) 0.0364(10) 0.0027(8) 0.0135(8) 0.0023(8)
C6 0.0333(10) 0.0283(11) 0.0368(10) 0.0030(8) 0.0120(8) -0.0001(8)
C7 0.0292(10) 0.0273(10) 0.0401(10) 0.0006(8) 0.0115(8) 0.0013(8)
C8 0.0310(10) 0.0248(10) 0.0425(10) -0.0003(8) 0.0145(8) 0.0013(8)
C9 0.0330(10) 0.0276(11) 0.0406(10) -0.0022(8) 0.0108(8) 0.0006(8)
C10 0.0330(10) 0.0306(11) 0.0370(10) -0.0021(8) 0.0103(8) -0.0007(8)
C11 0.0316(10) 0.0290(11) 0.0367(10) -0.0018(8) 0.0113(8) 0.0016(8)
C12 0.0313(10) 0.0324(11) 0.0349(10) 0.0002(8) 0.0121(8) 0.0023(8)
C13 0.0331(10) 0.0316(10) 0.0378(10) 0.0025(8) 0.0142(8) 0.0050(8)
C14 0.0340(10) 0.0269(10) 0.0411(10) 0.0021(8) 0.0157(9) 0.0032(8)
C15 0.0365(11) 0.0290(11) 0.0435(11) 0.0016(8) 0.0173(9) -0.0019(8)
C16 0.0326(10) 0.0311(11) 0.0428(10) -0.0018(8) 0.0144(9) -0.0006(8)
C17 0.0384(11) 0.0374(12) 0.0441(11) -0.0007(9) 0.0115(9) -0.0059(9)
C18 0.0362(11) 0.0339(11) 0.0397(11) 0.0016(8) 0.0094(9) -0.0008(9)
C19 0.0403(12) 0.0414(12) 0.0361(10) 0.0009(8) 0.0110(9) -0.0028(9)
C20 0.0509(13) 0.0446(13) 0.0441(11) -0.0049(9) 0.0162(10) -0.0015(10)
C21 0.0600(15) 0.0625(16) 0.0546(13) -0.0065(11) 0.0199(12) 0.0085(12)
C22 0.0345(11) 0.0274(11) 0.0421(10) 0.0016(8) 0.0102(9) -0.0007(8)
C23 0.0512(13) 0.0387(12) 0.0462(11) 0.0048(9) 0.0193(10) 0.0008(10)
C24 0.0332(10) 0.0280(11) 0.0428(10) -0.0014(8) 0.0134(9) -0.0004(8)
C25 0.0370(11) 0.0363(12) 0.0632(13) -0.0043(10) 0.0119(10) -0.0025(9)
C26 0.0417(11) 0.0349(11) 0.0373(10) 0.0005(8) 0.0137(9) 0.0003(9)
C27 0.0380(11) 0.0427(13) 0.0385(10) 0.0015(9) 0.0099(9) -0.0007(9)
C28 0.0486(13) 0.0430(13) 0.0477(12) 0.0053(9) 0.0137(10) 0.0057(10)
C29 0.0542(14) 0.0623(16) 0.0593(14) 0.0032(11) 0.0180(12) 0.0169(12)
C30 0.0416(12) 0.0391(12) 0.0421(11) 0.0031(9) 0.0157(9) -0.0017(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.351(2) . ?
N1 C4 1.362(2) . ?
N1 H1 0.8800 . ?
N2 C9 1.344(2) . ?
N2 C6 1.345(2) . ?
N3 C14 1.351(2) . ?
N3 C11 1.364(2) . ?
N3 H3 0.8800 . ?
C1 C16 1.413(2) . ?
C1 C2 1.459(2) . ?
C2 C3 1.374(2) . ?
C2 C17 1.495(2) . ?
C3 C4 1.457(2) . ?
C3 C18 1.501(2) . ?
C4 C5 1.403(2) . ?
C5 C6 1.408(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.475(2) . ?
C7 C8 1.368(2) . ?
C7 C22 1.493(2) . ?
C8 C9 1.480(2) . ?
C8 C24 1.495(2) . ?
C9 C10 1.406(2) . ?
C10 C11 1.407(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.462(2) . ?
C12 C13 1.373(2) . ?
C12 C26 1.502(2) . ?
C13 C14 1.464(2) . ?
C13 C30 1.497(2) . ?
C14 C15 1.417(2) . ?
C15 C16 1.395(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.536(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.520(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.525(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.525(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.522(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.542(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.515(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.522(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C4 110.23(15) . . ?
C1 N1 H1 124.9 . . ?
C4 N1 H1 124.9 . . ?
C9 N2 C6 108.46(16) . . ?
C14 N3 C11 109.78(16) . . ?
C14 N3 H3 125.1 . . ?
C11 N3 H3 125.1 . . ?
N1 C1 C16 122.90(16) . . ?
N1 C1 C2 108.20(15) . . ?
C16 C1 C2 128.87(16) . . ?
C3 C2 C1 106.69(16) . . ?
C3 C2 C17 128.63(17) . . ?
C1 C2 C17 124.67(16) . . ?
C2 C3 C4 107.27(16) . . ?
C2 C3 C18 129.13(17) . . ?
C4 C3 C18 123.50(16) . . ?
N1 C4 C5 123.24(16) . . ?
N1 C4 C3 107.60(16) . . ?
C5 C4 C3 129.14(16) . . ?
C4 C5 C6 121.94(16) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
N2 C6 C5 115.79(16) . . ?
N2 C6 C7 109.79(15) . . ?
C5 C6 C7 134.12(16) . . ?
C8 C7 C6 105.87(15) . . ?
C8 C7 C22 129.04(17) . . ?
C6 C7 C22 125.08(15) . . ?
C7 C8 C9 106.12(16) . . ?
C7 C8 C24 128.44(16) . . ?
C9 C8 C24 125.38(16) . . ?
N2 C9 C10 116.47(16) . . ?
N2 C9 C8 109.43(16) . . ?
C10 C9 C8 133.74(17) . . ?
C9 C10 C11 121.81(16) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
N3 C11 C10 122.68(16) . . ?
N3 C11 C12 107.91(16) . . ?
C10 C11 C12 129.40(16) . . ?
C13 C12 C11 107.15(15) . . ?
C13 C12 C26 129.26(16) . . ?
C11 C12 C26 123.57(16) . . ?
C12 C13 C14 106.53(15) . . ?
C12 C13 C30 128.90(16) . . ?
C14 C13 C30 124.56(16) . . ?
N3 C14 C15 122.88(17) . . ?
N3 C14 C13 108.60(16) . . ?
C15 C14 C13 128.52(17) . . ?
C16 C15 C14 131.45(17) . . ?
C16 C15 H15 114.3 . . ?
C14 C15 H15 114.3 . . ?
C15 C16 C1 131.74(17) . . ?
C15 C16 H16 114.1 . . ?
C1 C16 H16 114.1 . . ?
C2 C17 H17A 109.5 . . ?
C2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C3 C18 C19 113.43(15) . . ?
C3 C18 H18A 108.9 . . ?
C19 C18 H18A 108.9 . . ?
C3 C18 H18B 108.9 . . ?
C19 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C20 C19 C18 113.34(16) . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 C21 113.91(18) . . ?
C19 C20 H20A 108.8 . . ?
C21 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C22 C23 112.87(15) . . ?
C7 C22 H22A 109.0 . . ?
C23 C22 H22A 109.0 . . ?
C7 C22 H22B 109.0 . . ?
C23 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C8 C24 C25 111.45(15) . . ?
C8 C24 H24A 109.3 . . ?
C25 C24 H24A 109.3 . . ?
C8 C24 H24B 109.3 . . ?
C25 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C12 C26 C27 113.92(15) . . ?
C12 C26 H26A 108.8 . . ?
C27 C26 H26A 108.8 . . ?
C12 C26 H26B 108.8 . . ?
C27 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
C28 C27 C26 113.45(16) . . ?
C28 C27 H27A 108.9 . . ?
C26 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C26 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 C29 113.39(18) . . ?
C27 C28 H28A 108.9 . . ?
C29 C28 H28A 108.9 . . ?
C27 C28 H28B 108.9 . . ?
C29 C28 H28B 108.9 . . ?
H28A C28 H28B 107.7 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C13 C30 H30A 109.5 . . ?
C13 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C13 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 C1 C16 -177.10(16) . . . . ?
C4 N1 C1 C2 1.04(19) . . . . ?
N1 C1 C2 C3 -0.49(19) . . . . ?
C16 C1 C2 C3 177.50(18) . . . . ?
N1 C1 C2 C17 178.29(16) . . . . ?
C16 C1 C2 C17 -3.7(3) . . . . ?
C1 C2 C3 C4 -0.21(19) . . . . ?
C17 C2 C3 C4 -178.93(17) . . . . ?
C1 C2 C3 C18 -176.53(17) . . . . ?
C17 C2 C3 C18 4.8(3) . . . . ?
C1 N1 C4 C5 177.40(16) . . . . ?
C1 N1 C4 C3 -1.2(2) . . . . ?
C2 C3 C4 N1 0.8(2) . . . . ?
C18 C3 C4 N1 177.41(15) . . . . ?
C2 C3 C4 C5 -177.62(18) . . . . ?
C18 C3 C4 C5 -1.0(3) . . . . ?
N1 C4 C5 C6 -4.8(3) . . . . ?
C3 C4 C5 C6 173.44(17) . . . . ?
C9 N2 C6 C5 168.72(16) . . . . ?
C9 N2 C6 C7 -5.8(2) . . . . ?
C4 C5 C6 N2 -8.0(3) . . . . ?
C4 C5 C6 C7 164.80(18) . . . . ?
N2 C6 C7 C8 3.7(2) . . . . ?
C5 C6 C7 C8 -169.5(2) . . . . ?
N2 C6 C7 C22 -176.07(15) . . . . ?
C5 C6 C7 C22 10.8(3) . . . . ?
C6 C7 C8 C9 -0.20(18) . . . . ?
C22 C7 C8 C9 179.52(17) . . . . ?
C6 C7 C8 C24 -177.49(16) . . . . ?
C22 C7 C8 C24 2.2(3) . . . . ?
C6 N2 C9 C10 -168.42(15) . . . . ?
C6 N2 C9 C8 5.7(2) . . . . ?
C7 C8 C9 N2 -3.3(2) . . . . ?
C24 C8 C9 N2 174.08(16) . . . . ?
C7 C8 C9 C10 169.36(19) . . . . ?
C24 C8 C9 C10 -13.2(3) . . . . ?
N2 C9 C10 C11 7.2(3) . . . . ?
C8 C9 C10 C11 -165.11(18) . . . . ?
C14 N3 C11 C10 -177.32(16) . . . . ?
C14 N3 C11 C12 1.8(2) . . . . ?
C9 C10 C11 N3 5.0(3) . . . . ?
C9 C10 C11 C12 -173.98(17) . . . . ?
N3 C11 C12 C13 -1.8(2) . . . . ?
C10 C11 C12 C13 177.26(17) . . . . ?
N3 C11 C12 C26 179.46(15) . . . . ?
C10 C11 C12 C26 -1.5(3) . . . . ?
C11 C12 C13 C14 1.09(19) . . . . ?
C26 C12 C13 C14 179.71(17) . . . . ?
C11 C12 C13 C30 179.69(17) . . . . ?
C26 C12 C13 C30 -1.7(3) . . . . ?
C11 N3 C14 C15 178.69(16) . . . . ?
C11 N3 C14 C13 -1.2(2) . . . . ?
C12 C13 C14 N3 -0.01(19) . . . . ?
C30 C13 C14 N3 -178.69(16) . . . . ?
C12 C13 C14 C15 -179.85(17) . . . . ?
C30 C13 C14 C15 1.5(3) . . . . ?
N3 C14 C15 C16 -2.1(3) . . . . ?
C13 C14 C15 C16 177.75(18) . . . . ?
C14 C15 C16 C1 0.1(3) . . . . ?
N1 C1 C16 C15 1.7(3) . . . . ?
C2 C1 C16 C15 -176.02(18) . . . . ?
C2 C3 C18 C19 95.5(2) . . . . ?
C4 C3 C18 C19 -80.3(2) . . . . ?
C3 C18 C19 C20 -72.1(2) . . . . ?
C18 C19 C20 C21 -176.75(16) . . . . ?
C8 C7 C22 C23 -103.2(2) . . . . ?
C6 C7 C22 C23 76.5(2) . . . . ?
C7 C8 C24 C25 96.5(2) . . . . ?
C9 C8 C24 C25 -80.3(2) . . . . ?
C13 C12 C26 C27 -98.1(2) . . . . ?
C11 C12 C26 C27 80.3(2) . . . . ?
C12 C26 C27 C28 74.2(2) . . . . ?
C26 C27 C28 C29 178.93(17) . . . . ?

# Attachment '- TriphyrinMn.cif'

data___kuzuhara
_database_code_depnum_ccdc_archive 'CCDC 790489'
#TrackingRef '- TriphyrinMn.cif'

#==============================================================================

# CHEMICAL DATA

_chemical_formula_sum            'C33 H38 Mn N3 O3 '
_chemical_formula_moiety         'C33 H38 Mn N3 O3 '
_chemical_formula_weight         579.62
_chemical_melting_point          ?

#==============================================================================

# CRYSTAL DATA
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.844(2)
_cell_length_b                   15.867(3)
_cell_length_c                   17.615(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.781(3)
_cell_angle_gamma                90.00
_cell_volume                     2986.8(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8824
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      31.1

#------------------------------------------------------------------------------

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_T_max  0.953
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'VariMax 50 kV 24 mA Rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            48856
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         27.48
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999

#==============================================================================

_computing_data_collection       CrystalClear
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_solution    SIR2004
_computing_structure_refinement  SHELXL97
_computing_publication_material  'CrystalStructure 3.8.2'
_computing_molecular_graphics    ?

#==============================================================================
_reflns_number_total             6835
_reflns_number_gt                6371
_reflns_threshold_expression     >2sigma(I)
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. One of the butyl groups
disordered. Their atomic ccordinates were restrained by SAME, ISOR, DELU,
and SIMU commands. Coordination of carbon monooxide groups to manganese(I)
were rather weak. Therefore, the thermal movements of the groups were
random and the Hirshfeld alerts for this phenomena were created.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+2.0940P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6835
_refine_ls_number_parameters     389
_refine_ls_number_restraints     128
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.1069
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.062

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.35190(3) 0.646721(17) 0.679461(15) 0.01311(9) Uani 1 1 d . . .
O1 O 0.18604(14) 0.54009(9) 0.75702(9) 0.0260(3) Uani 1 1 d . . .
O2 O 0.11863(14) 0.72592(11) 0.59824(9) 0.0340(4) Uani 1 1 d . . .
O3 O 0.33999(15) 0.76636(9) 0.80616(8) 0.0270(3) Uani 1 1 d . . .
N1 N 0.36936(14) 0.57059(9) 0.59102(8) 0.0146(3) Uani 1 1 d . . .
N2 N 0.46626(14) 0.71668(9) 0.62894(8) 0.0137(3) Uani 1 1 d . A .
N3 N 0.51489(14) 0.59618(9) 0.72909(8) 0.0142(3) Uani 1 1 d . A .
C1 C 0.35718(17) 0.48584(11) 0.58833(10) 0.0155(4) Uani 1 1 d . . .
C2 C 0.31562(18) 0.45947(12) 0.50853(11) 0.0177(4) Uani 1 1 d . A .
C3 C 0.31208(17) 0.53014(12) 0.46427(10) 0.0165(4) Uani 1 1 d D . .
C4 C 0.34973(17) 0.60028(11) 0.51669(10) 0.0148(4) Uani 1 1 d . A .
C5 C 0.38041(17) 0.68262(11) 0.49845(10) 0.0154(4) Uani 1 1 d . . .
H5 H 0.3543 0.7025 0.4474 0.019 Uiso 1 1 calc R A .
C6 C 0.44862(17) 0.73709(11) 0.55320(10) 0.0150(4) Uani 1 1 d . A .
C7 C 0.53623(17) 0.80446(11) 0.54166(10) 0.0162(4) Uani 1 1 d . . .
C8 C 0.61212(17) 0.81671(11) 0.61146(11) 0.0162(4) Uani 1 1 d . A .
C9 C 0.57020(17) 0.75693(11) 0.66501(10) 0.0148(3) Uani 1 1 d . . .
C10 C 0.63572(17) 0.72558(11) 0.73519(10) 0.0155(4) Uani 1 1 d . A .
H10 H 0.6969 0.7603 0.7650 0.019 Uiso 1 1 calc R . .
C11 C 0.61396(17) 0.64500(11) 0.76263(10) 0.0149(4) Uani 1 1 d . . .
C12 C 0.69825(17) 0.59397(12) 0.81732(10) 0.0169(4) Uani 1 1 d . A .
C13 C 0.65163(17) 0.51363(12) 0.81112(10) 0.0171(4) Uani 1 1 d . . .
C14 C 0.53749(17) 0.51601(11) 0.75348(10) 0.0150(4) Uani 1 1 d . A .
C15 C 0.47041(17) 0.44470(12) 0.72245(10) 0.0167(4) Uani 1 1 d . . .
H15 H 0.4795 0.3969 0.7554 0.020 Uiso 1 1 calc R A .
C16 C 0.39284(17) 0.43165(12) 0.65182(11) 0.0177(4) Uani 1 1 d . A .
H16 H 0.3579 0.3767 0.6453 0.021 Uiso 1 1 calc R . .
C17 C 0.2852(2) 0.37130(12) 0.48154(12) 0.0236(4) Uani 1 1 d . . .
H17A H 0.1956 0.3609 0.4793 0.035 Uiso 1 1 calc R A .
H17B H 0.3333 0.3315 0.5175 0.035 Uiso 1 1 calc R . .
H17C H 0.3069 0.3637 0.4302 0.035 Uiso 1 1 calc R . .
C18 C 0.27442(19) 0.53548(13) 0.37863(11) 0.0213(4) Uani 0.799(5) 1 d PDU A 1
H18A H 0.3081 0.4861 0.3546 0.026 Uiso 0.799(5) 1 calc PR A 1
H18B H 0.3115 0.5868 0.3597 0.026 Uiso 0.799(5) 1 calc PR A 1
C19 C 0.1307(2) 0.53825(19) 0.35385(14) 0.0215(6) Uani 0.799(5) 1 d PDU A 1
H19A H 0.1101 0.5351 0.2970 0.026 Uiso 0.799(5) 1 calc PR A 1
H19B H 0.0934 0.4885 0.3752 0.026 Uiso 0.799(5) 1 calc PR A 1
C20 C 0.0738(2) 0.61780(17) 0.38117(17) 0.0273(7) Uani 0.799(5) 1 d PDU A 1
H20A H 0.1123 0.6675 0.3605 0.033 Uiso 0.799(5) 1 calc PR A 1
H20B H 0.0937 0.6205 0.4381 0.033 Uiso 0.799(5) 1 calc PR A 1
C21 C -0.0680(4) 0.6221(3) 0.3562(4) 0.0376(11) Uani 0.799(5) 1 d PDU A 1
H21A H -0.0884 0.6204 0.2999 0.056 Uiso 0.799(5) 1 calc PR A 1
H21B H -0.0995 0.6747 0.3750 0.056 Uiso 0.799(5) 1 calc PR A 1
H21C H -0.1070 0.5740 0.3778 0.056 Uiso 0.799(5) 1 calc PR A 1
C18A C 0.27442(19) 0.53548(13) 0.37863(11) 0.0213(4) Uani 0.201(5) 1 d PD A 2
H18C H 0.2578 0.4782 0.3570 0.026 Uiso 0.201(5) 1 calc PR A 2
H18D H 0.3434 0.5604 0.3558 0.026 Uiso 0.201(5) 1 calc PR A 2
C19A C 0.1525(9) 0.5918(8) 0.3574(6) 0.027(3) Uani 0.201(5) 1 d PDU A 2
H19C H 0.1644 0.6469 0.3840 0.032 Uiso 0.201(5) 1 calc PR A 2
H19D H 0.1337 0.6019 0.3011 0.032 Uiso 0.201(5) 1 calc PR A 2
C20A C 0.0460(10) 0.5428(7) 0.3838(7) 0.033(3) Uani 0.201(5) 1 d PDU A 2
H20C H 0.0285 0.4911 0.3524 0.040 Uiso 0.201(5) 1 calc PR A 2
H20D H 0.0714 0.5258 0.4382 0.040 Uiso 0.201(5) 1 calc PR A 2
C21A C -0.0724(18) 0.5966(16) 0.3758(18) 0.053(6) Uani 0.201(5) 1 d PDU A 2
H21D H -0.0516 0.6522 0.3987 0.079 Uiso 0.201(5) 1 calc PR A 2
H21E H -0.1337 0.5689 0.4024 0.079 Uiso 0.201(5) 1 calc PR A 2
H21F H -0.1079 0.6031 0.3211 0.079 Uiso 0.201(5) 1 calc PR A 2
C22 C 0.54343(18) 0.84627(12) 0.46626(11) 0.0185(4) Uani 1 1 d . A .
H22A H 0.5522 0.8024 0.4276 0.022 Uiso 1 1 calc R . .
H22B H 0.6192 0.8822 0.4724 0.022 Uiso 1 1 calc R . .
C23 C 0.42894(19) 0.90042(13) 0.43622(12) 0.0240(4) Uani 1 1 d . . .
H23A H 0.3540 0.8648 0.4274 0.036 Uiso 1 1 calc R A .
H23B H 0.4400 0.9273 0.3877 0.036 Uiso 1 1 calc R . .
H23C H 0.4193 0.9439 0.4743 0.036 Uiso 1 1 calc R . .
C24 C 0.72483(18) 0.87224(12) 0.63028(11) 0.0204(4) Uani 1 1 d . . .
H24A H 0.7338 0.8899 0.6848 0.025 Uiso 1 1 calc R A .
H24B H 0.7116 0.9236 0.5980 0.025 Uiso 1 1 calc R . .
C25 C 0.8461(2) 0.82946(15) 0.61738(14) 0.0305(5) Uani 1 1 d . A .
H25A H 0.8596 0.7782 0.6488 0.046 Uiso 1 1 calc R . .
H25B H 0.9166 0.8681 0.6323 0.046 Uiso 1 1 calc R . .
H25C H 0.8399 0.8147 0.5628 0.046 Uiso 1 1 calc R . .
C26 C 0.81466(18) 0.62481(13) 0.86789(11) 0.0200(4) Uani 1 1 d . . .
H26A H 0.8300 0.5895 0.9149 0.024 Uiso 1 1 calc R A .
H26B H 0.8001 0.6832 0.8841 0.024 Uiso 1 1 calc R . .
C27 C 0.93258(19) 0.62390(15) 0.83093(12) 0.0254(4) Uani 1 1 d . A .
H27A H 0.9456 0.5663 0.8123 0.031 Uiso 1 1 calc R . .
H27B H 0.9202 0.6621 0.7858 0.031 Uiso 1 1 calc R . .
C28 C 1.0493(2) 0.65120(14) 0.88653(13) 0.0277(5) Uani 1 1 d . . .
H28A H 1.1186 0.6592 0.8572 0.033 Uiso 1 1 calc R A .
H28B H 1.0327 0.7063 0.9092 0.033 Uiso 1 1 calc R . .
C29 C 1.0904(2) 0.5893(2) 0.95094(16) 0.0503(8) Uani 1 1 d . A .
H29A H 1.0236 0.5826 0.9816 0.075 Uiso 1 1 calc R . .
H29B H 1.1660 0.6105 0.9839 0.075 Uiso 1 1 calc R . .
H29C H 1.1083 0.5347 0.9291 0.075 Uiso 1 1 calc R . .
C30 C 0.7081(2) 0.43530(13) 0.84993(12) 0.0242(4) Uani 1 1 d . A .
H30A H 0.7356 0.3982 0.8116 0.036 Uiso 1 1 calc R . .
H30B H 0.6456 0.4061 0.8744 0.036 Uiso 1 1 calc R . .
H30C H 0.7801 0.4504 0.8891 0.036 Uiso 1 1 calc R . .
C31 C 0.25348(18) 0.57772(12) 0.72589(11) 0.0181(4) Uani 1 1 d . . .
C32 C 0.20977(19) 0.69506(12) 0.62784(11) 0.0200(4) Uani 1 1 d . . .
C33 C 0.34752(17) 0.71957(12) 0.75702(10) 0.0171(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.01539(15) 0.01244(14) 0.01154(14) -0.00068(10) 0.00240(10) 0.00129(10)
O1 0.0273(8) 0.0218(7) 0.0316(8) 0.0034(6) 0.0129(6) -0.0015(6)
O2 0.0249(8) 0.0428(10) 0.0326(9) 0.0053(7) -0.0005(7) 0.0143(7)
O3 0.0402(9) 0.0225(7) 0.0195(7) -0.0068(6) 0.0089(6) 0.0014(6)
N1 0.0171(8) 0.0136(7) 0.0126(7) -0.0001(6) 0.0008(6) 0.0017(6)
N2 0.0171(7) 0.0128(7) 0.0112(7) -0.0006(6) 0.0021(6) 0.0016(6)
N3 0.0178(8) 0.0132(7) 0.0118(7) -0.0002(6) 0.0029(6) 0.0015(6)
C1 0.0155(9) 0.0143(8) 0.0165(9) -0.0021(7) 0.0022(7) 0.0004(7)
C2 0.0181(9) 0.0160(9) 0.0185(9) -0.0049(7) 0.0014(7) 0.0023(7)
C3 0.0144(9) 0.0199(9) 0.0151(9) -0.0047(7) 0.0024(7) 0.0011(7)
C4 0.0154(9) 0.0164(9) 0.0125(8) -0.0018(7) 0.0024(7) 0.0035(7)
C5 0.0164(9) 0.0172(9) 0.0124(8) 0.0009(7) 0.0015(7) 0.0026(7)
C6 0.0177(9) 0.0137(8) 0.0141(8) 0.0015(7) 0.0038(7) 0.0042(7)
C7 0.0187(9) 0.0136(8) 0.0174(9) 0.0005(7) 0.0061(7) 0.0038(7)
C8 0.0180(9) 0.0130(8) 0.0181(9) -0.0014(7) 0.0046(7) 0.0021(7)
C9 0.0173(9) 0.0135(8) 0.0141(8) -0.0022(7) 0.0046(7) 0.0001(7)
C10 0.0181(9) 0.0150(9) 0.0133(8) -0.0040(7) 0.0024(7) -0.0012(7)
C11 0.0166(9) 0.0175(9) 0.0106(8) -0.0018(7) 0.0024(7) 0.0010(7)
C12 0.0180(9) 0.0216(9) 0.0116(8) 0.0012(7) 0.0039(7) 0.0030(7)
C13 0.0179(9) 0.0204(9) 0.0128(8) 0.0021(7) 0.0022(7) 0.0016(7)
C14 0.0165(9) 0.0163(9) 0.0126(8) 0.0014(7) 0.0036(7) 0.0030(7)
C15 0.0195(9) 0.0146(9) 0.0170(9) 0.0042(7) 0.0055(7) 0.0028(7)
C16 0.0184(9) 0.0140(9) 0.0209(9) -0.0015(7) 0.0037(7) 0.0000(7)
C17 0.0281(11) 0.0182(9) 0.0227(10) -0.0067(8) -0.0009(8) 0.0012(8)
C18 0.0222(10) 0.0286(11) 0.0131(9) -0.0033(7) 0.0028(7) 0.0018(8)
C19 0.0218(13) 0.0233(15) 0.0177(12) -0.0034(10) -0.0016(10) -0.0018(10)
C20 0.0204(14) 0.0257(14) 0.0338(15) -0.0057(11) -0.0014(11) -0.0007(11)
C21 0.0227(18) 0.035(3) 0.052(3) -0.0060(19) -0.0030(16) 0.0047(16)
C18A 0.0222(10) 0.0286(11) 0.0131(9) -0.0033(7) 0.0028(7) 0.0018(8)
C19A 0.030(5) 0.027(6) 0.022(5) -0.001(4) -0.002(4) 0.003(4)
C20A 0.026(5) 0.038(6) 0.035(6) -0.003(5) 0.002(4) -0.002(4)
C21A 0.026(7) 0.057(14) 0.074(15) -0.015(10) 0.004(8) 0.005(8)
C22 0.0210(9) 0.0188(9) 0.0169(9) 0.0032(7) 0.0065(7) 0.0014(7)
C23 0.0251(10) 0.0248(10) 0.0224(10) 0.0067(8) 0.0048(8) 0.0033(8)
C24 0.0216(10) 0.0188(9) 0.0212(9) 0.0005(7) 0.0043(8) -0.0018(8)
C25 0.0213(11) 0.0311(12) 0.0398(13) -0.0016(10) 0.0077(9) -0.0012(9)
C26 0.0199(9) 0.0247(10) 0.0149(9) -0.0002(7) 0.0017(7) 0.0003(8)
C27 0.0199(10) 0.0371(12) 0.0195(10) 0.0001(9) 0.0039(8) 0.0002(9)
C28 0.0192(10) 0.0338(12) 0.0305(11) -0.0008(9) 0.0049(9) -0.0028(8)
C29 0.0198(12) 0.089(2) 0.0400(15) 0.0224(15) -0.0004(10) 0.0037(13)
C30 0.0254(10) 0.0230(10) 0.0223(10) 0.0050(8) -0.0015(8) 0.0023(8)
C31 0.0199(9) 0.0162(9) 0.0174(9) -0.0023(7) 0.0006(7) 0.0041(7)
C32 0.0240(10) 0.0201(9) 0.0170(9) -0.0007(7) 0.0067(8) 0.0006(8)
C33 0.0189(9) 0.0163(9) 0.0162(9) 0.0037(7) 0.0030(7) 0.0003(7)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 C33 1.7964(19) . ?
Mn1 C31 1.817(2) . ?
Mn1 C32 1.821(2) . ?
Mn1 N2 1.9841(16) . ?
Mn1 N3 2.0015(16) . ?
Mn1 N1 2.0056(15) . ?
O1 C31 1.152(2) . ?
O2 C32 1.146(2) . ?
O3 C33 1.154(2) . ?
N1 C1 1.351(2) . ?
N1 C4 1.374(2) . ?
N2 C6 1.355(2) . ?
N2 C9 1.356(2) . ?
N3 C14 1.352(2) . ?
N3 C11 1.374(2) . ?
C1 C16 1.412(3) . ?
C1 C2 1.463(2) . ?
C2 C3 1.362(3) . ?
C2 C17 1.496(3) . ?
C3 C4 1.459(2) . ?
C3 C18 1.497(3) . ?
C4 C5 1.399(3) . ?
C5 C6 1.408(3) . ?
C6 C7 1.467(3) . ?
C7 C8 1.372(3) . ?
C7 C22 1.499(3) . ?
C8 C9 1.463(3) . ?
C8 C24 1.497(3) . ?
C9 C10 1.408(2) . ?
C10 C11 1.401(3) . ?
C11 C12 1.456(2) . ?
C12 C13 1.369(3) . ?
C12 C26 1.498(3) . ?
C13 C14 1.462(3) . ?
C13 C30 1.498(3) . ?
C14 C15 1.405(3) . ?
C15 C16 1.394(3) . ?
C18 C19 1.546(3) . ?
C19 C20 1.519(4) . ?
C20 C21 1.527(5) . ?
C19A C20A 1.528(13) . ?
C20A C21A 1.528(15) . ?
C22 C23 1.529(3) . ?
C24 C25 1.531(3) . ?
C26 C27 1.530(3) . ?
C27 C28 1.525(3) . ?
C28 C29 1.509(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C33 Mn1 C31 87.25(8) . . ?
C33 Mn1 C32 88.81(8) . . ?
C31 Mn1 C32 88.08(9) . . ?
C33 Mn1 N2 94.62(7) . . ?
C31 Mn1 N2 176.73(7) . . ?
C32 Mn1 N2 94.64(8) . . ?
C33 Mn1 N3 93.50(7) . . ?
C31 Mn1 N3 96.00(7) . . ?
C32 Mn1 N3 175.39(7) . . ?
N2 Mn1 N3 81.21(6) . . ?
C33 Mn1 N1 175.22(8) . . ?
C31 Mn1 N1 97.29(7) . . ?
C32 Mn1 N1 92.83(7) . . ?
N2 Mn1 N1 80.78(6) . . ?
N3 Mn1 N1 84.56(6) . . ?
C1 N1 C4 108.02(15) . . ?
C1 N1 Mn1 127.24(13) . . ?
C4 N1 Mn1 120.94(12) . . ?
C6 N2 C9 108.41(15) . . ?
C6 N2 Mn1 125.54(12) . . ?
C9 N2 Mn1 125.90(12) . . ?
C14 N3 C11 107.92(15) . . ?
C14 N3 Mn1 127.94(13) . . ?
C11 N3 Mn1 122.00(12) . . ?
N1 C1 C16 124.50(17) . . ?
N1 C1 C2 109.32(16) . . ?
C16 C1 C2 125.83(17) . . ?
C3 C2 C1 106.78(16) . . ?
C3 C2 C17 127.19(17) . . ?
C1 C2 C17 126.03(17) . . ?
C2 C3 C4 106.73(16) . . ?
C2 C3 C18 126.85(17) . . ?
C4 C3 C18 126.41(17) . . ?
N1 C4 C5 122.33(16) . . ?
N1 C4 C3 108.84(16) . . ?
C5 C4 C3 128.23(17) . . ?
C4 C5 C6 122.27(16) . . ?
N2 C6 C5 119.85(16) . . ?
N2 C6 C7 108.93(16) . . ?
C5 C6 C7 129.03(16) . . ?
C8 C7 C6 106.44(16) . . ?
C8 C7 C22 128.16(18) . . ?
C6 C7 C22 125.30(17) . . ?
C7 C8 C9 106.32(16) . . ?
C7 C8 C24 128.63(17) . . ?
C9 C8 C24 124.75(17) . . ?
N2 C9 C10 120.02(16) . . ?
N2 C9 C8 109.13(15) . . ?
C10 C9 C8 129.00(17) . . ?
C11 C10 C9 122.41(17) . . ?
N3 C11 C10 122.09(16) . . ?
N3 C11 C12 109.16(16) . . ?
C10 C11 C12 127.75(17) . . ?
C13 C12 C11 106.45(16) . . ?
C13 C12 C26 127.89(17) . . ?
C11 C12 C26 125.63(17) . . ?
C12 C13 C14 106.80(16) . . ?
C12 C13 C30 128.26(17) . . ?
C14 C13 C30 124.79(17) . . ?
N3 C14 C15 125.48(16) . . ?
N3 C14 C13 109.36(16) . . ?
C15 C14 C13 124.80(16) . . ?
C16 C15 C14 131.38(17) . . ?
C15 C16 C1 131.24(18) . . ?
C3 C18 C19 112.06(17) . . ?
C20 C19 C18 112.2(2) . . ?
C19 C20 C21 112.9(3) . . ?
C21A C20A C19A 110.8(12) . . ?
C7 C22 C23 113.21(16) . . ?
C8 C24 C25 113.31(17) . . ?
C12 C26 C27 115.12(16) . . ?
C28 C27 C26 112.71(17) . . ?
C29 C28 C27 113.9(2) . . ?
O1 C31 Mn1 174.14(17) . . ?
O2 C32 Mn1 177.13(17) . . ?
O3 C33 Mn1 177.49(17) . . ?

# Attachment '- TriphyrinRe.cif'

data___kuzuhara_1
_database_code_depnum_ccdc_archive 'CCDC 794381'
#TrackingRef '- TriphyrinRe.cif'

#==============================================================================

# CHEMICAL DATA

_chemical_formula_sum            'C33 H38 N3 O3 Re '
_chemical_formula_moiety         'C33 H38 N3 O3 Re '
_chemical_formula_weight         710.87

#==============================================================================

# CRYSTAL DATA
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1361(17)
_cell_length_b                   10.5681(18)
_cell_length_c                   13.789(2)
_cell_angle_alpha                87.855(4)
_cell_angle_beta                 87.178(5)
_cell_angle_gamma                84.036(6)
_cell_volume                     1466.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5583
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      31.1

#------------------------------------------------------------------------------

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    4.181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_correction_T_min  0.546
_exptl_absorpt_correction_T_max  0.605
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'VariMax 50 kV 24 mA Rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            24082
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         27.48
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998

#==============================================================================

_computing_data_collection       CrystalClear
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_solution    SIR2004
_computing_structure_refinement  SHELXL
_computing_publication_material  'CrystalStructure 3.8.2'
_computing_molecular_graphics    ?

#==============================================================================

_reflns_number_total             6703
_reflns_number_gt                6578
_reflns_threshold_expression     >2sigma(I)
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. Positional coordinates of
hydrogen atoms were refined either with restrain for alkyl groups or without
restrain for macrocyclic moiety.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+0.9677P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0049(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6703
_refine_ls_number_parameters     403
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0156
_refine_ls_wR_factor_ref         0.0389
_refine_ls_wR_factor_gt          0.0387
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.080

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.244503(6) 0.360127(6) 0.272465(4) 0.00855(4) Uani 1 1 d . . .
O1 O 0.34266(16) 0.08779(14) 0.34174(12) 0.0272(3) Uani 1 1 d . . .
O2 O 0.01601(14) 0.25616(14) 0.17089(10) 0.0203(3) Uani 1 1 d . . .
O3 O 0.06004(15) 0.36313(15) 0.45722(10) 0.0213(3) Uani 1 1 d . . .
N1 N 0.38146(15) 0.36175(14) 0.15026(11) 0.0098(3) Uani 1 1 d . . .
N2 N 0.40141(15) 0.45516(14) 0.32432(11) 0.0103(3) Uani 1 1 d . . .
N3 N 0.19720(15) 0.55202(14) 0.22301(11) 0.0099(3) Uani 1 1 d . . .
C1 C 0.35767(18) 0.37212(16) 0.05421(13) 0.0102(3) Uani 1 1 d . . .
C2 C 0.47632(18) 0.31936(17) -0.00207(13) 0.0119(3) Uani 1 1 d . . .
C3 C 0.57041(18) 0.28225(17) 0.06345(13) 0.0114(3) Uani 1 1 d . . .
C4 C 0.51204(17) 0.31575(16) 0.15883(13) 0.0108(3) Uani 1 1 d . . .
C5 C 0.58250(18) 0.33184(17) 0.24167(13) 0.0122(3) Uani 1 1 d . . .
H5 H 0.676(2) 0.305(2) 0.2392(17) 0.015 Uiso 1 1 d . . .
C6 C 0.53288(18) 0.41460(17) 0.31524(13) 0.0110(3) Uani 1 1 d . . .
C7 C 0.60831(18) 0.49649(17) 0.36944(13) 0.0117(3) Uani 1 1 d . . .
C8 C 0.51871(18) 0.59268(18) 0.40332(13) 0.0124(3) Uani 1 1 d . . .
C9 C 0.38959(18) 0.56816(17) 0.36975(12) 0.0111(3) Uani 1 1 d . . .
C10 C 0.27866(18) 0.65792(18) 0.35831(13) 0.0119(3) Uani 1 1 d . . .
H10 H 0.273(2) 0.732(2) 0.3909(17) 0.014 Uiso 1 1 d . . .
C11 C 0.19232(17) 0.65391(17) 0.28263(13) 0.0112(3) Uani 1 1 d . . .
C12 C 0.10873(17) 0.76047(17) 0.24041(13) 0.0122(3) Uani 1 1 d . . .
C13 C 0.06945(17) 0.72033(17) 0.15396(13) 0.0119(3) Uani 1 1 d . . .
C14 C 0.13284(17) 0.59105(17) 0.14171(13) 0.0106(3) Uani 1 1 d . . .
C15 C 0.14504(18) 0.52725(17) 0.05307(13) 0.0112(3) Uani 1 1 d . . .
H15 H 0.082(2) 0.565(2) 0.0077(17) 0.013 Uiso 1 1 d . . .
C16 C 0.24193(18) 0.43571(17) 0.01516(13) 0.0113(3) Uani 1 1 d . . .
H16 H 0.234(2) 0.424(2) -0.0528(17) 0.014 Uiso 1 1 d . . .
C17 C 0.4907(2) 0.31975(18) -0.11091(14) 0.0155(4) Uani 1 1 d . . .
H17A H 0.4980(15) 0.4029(12) -0.1350(4) 0.023 Uiso 1 1 d R . .
H17B H 0.4160(13) 0.2894(14) -0.1357(4) 0.023 Uiso 1 1 d R . .
H17C H 0.5669(14) 0.2672(14) -0.1299(3) 0.023 Uiso 1 1 d R . .
C18 C 0.71183(18) 0.22614(17) 0.04751(14) 0.0134(4) Uani 1 1 d . . .
H18A H 0.7697(10) 0.2824(10) 0.0735(5) 0.016 Uiso 1 1 d R . .
H18B H 0.7324(4) 0.22165(19) -0.0216(12) 0.016 Uiso 1 1 d R . .
C19 C 0.74121(19) 0.09285(18) 0.09444(15) 0.0161(4) Uani 1 1 d . . .
H19A H 0.8381(17) 0.0684(5) 0.08955(16) 0.019 Uiso 1 1 d R . .
H19B H 0.7139(5) 0.09611(19) 0.1642(12) 0.019 Uiso 1 1 d R . .
C20 C 0.6710(2) -0.00973(19) 0.04841(15) 0.0185(4) Uani 1 1 d . . .
H20A H 0.6879(3) -0.0902(14) 0.0864(7) 0.022 Uiso 1 1 d R . .
H20B H 0.5745(17) 0.0154(5) 0.05230(17) 0.022 Uiso 1 1 d R . .
C21 C 0.7148(2) -0.0329(2) -0.05752(16) 0.0231(4) Uani 1 1 d . . .
H21A H 0.6898(15) 0.0461(13) -0.0981(7) 0.035 Uiso 1 1 d R . .
H21B H 0.6698(14) -0.1054(15) -0.0814(5) 0.035 Uiso 1 1 d R . .
H21C H 0.8138(15) -0.0546(16) -0.0628(3) 0.035 Uiso 1 1 d R . .
C22 C 0.75638(18) 0.48076(19) 0.37582(14) 0.0153(4) Uani 1 1 d . . .
H22A H 0.7875(6) 0.3891(16) 0.37712(14) 0.018 Uiso 1 1 d R . .
H22B H 0.7795(4) 0.5156(6) 0.4375(11) 0.018 Uiso 1 1 d R . .
C23 C 0.8292(2) 0.5465(2) 0.29176(18) 0.0259(5) Uani 1 1 d . . .
H23A H 0.8107(14) 0.5086(13) 0.2298(10) 0.039 Uiso 1 1 d R . .
H23B H 0.9260(16) 0.5350(14) 0.3014(7) 0.039 Uiso 1 1 d R . .
H23C H 0.7981(14) 0.6386(15) 0.2895(8) 0.039 Uiso 1 1 d R . .
C24 C 0.5445(2) 0.70909(19) 0.45540(14) 0.0169(4) Uani 1 1 d . . .
H24A H 0.6233(14) 0.6908(4) 0.4900(7) 0.020 Uiso 1 1 d R . .
H24B H 0.4734(13) 0.7292(4) 0.5015(9) 0.020 Uiso 1 1 d R . .
C25 C 0.5592(2) 0.8251(2) 0.38745(17) 0.0258(5) Uani 1 1 d . . .
H25A H 0.6399(16) 0.8076(7) 0.3425(11) 0.039 Uiso 1 1 d R . .
H25B H 0.5696(18) 0.9013(13) 0.4270(6) 0.039 Uiso 1 1 d R . .
H25C H 0.4778(15) 0.8426(11) 0.3481(11) 0.039 Uiso 1 1 d R . .
C26 C 0.08134(19) 0.89117(18) 0.28117(14) 0.0148(4) Uani 1 1 d . . .
H26A H 0.08354(19) 0.9545(11) 0.2273(9) 0.018 Uiso 1 1 d R . .
H26B H 0.1529(12) 0.9046(3) 0.3239(7) 0.018 Uiso 1 1 d R . .
C27 C -0.05189(19) 0.91481(18) 0.33853(14) 0.0163(4) Uani 1 1 d . . .
H27A H -0.1237(13) 0.8997(3) 0.2973(7) 0.020 Uiso 1 1 d R . .
H27B H -0.0535(2) 0.8553(11) 0.3941(10) 0.020 Uiso 1 1 d R . .
C28 C -0.0739(2) 1.05087(19) 0.37391(16) 0.0203(4) Uani 1 1 d . . .
H28A H -0.0671(3) 1.1098(11) 0.3181(10) 0.024 Uiso 1 1 d R . .
H28B H -0.0035(13) 1.0641(3) 0.4171(8) 0.024 Uiso 1 1 d R . .
C29 C -0.2083(2) 1.0822(2) 0.42766(17) 0.0275(5) Uani 1 1 d . . .
H29A H -0.2794(12) 1.0734(17) 0.3840(8) 0.041 Uiso 1 1 d R . .
H29B H -0.2151(8) 1.1694(16) 0.4497(12) 0.041 Uiso 1 1 d R . .
H29C H -0.2161(8) 1.0237(15) 0.4836(12) 0.041 Uiso 1 1 d R . .
C30 C -0.01541(19) 0.79608(18) 0.08280(14) 0.0159(4) Uani 1 1 d . . .
H30A H -0.1043(14) 0.7827(11) 0.0962(7) 0.024 Uiso 1 1 d R . .
H30B H 0.0102(11) 0.7705(11) 0.0199(10) 0.024 Uiso 1 1 d R . .
H30C H -0.0053(12) 0.8825(13) 0.0877(8) 0.024 Uiso 1 1 d R . .
C31 C 0.30668(19) 0.18992(19) 0.31519(14) 0.0157(4) Uani 1 1 d . . .
C32 C 0.10316(19) 0.29351(18) 0.20873(13) 0.0134(4) Uani 1 1 d . . .
C33 C 0.12928(18) 0.36599(18) 0.38829(14) 0.0130(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.00769(5) 0.00840(5) 0.00973(5) -0.00010(3) -0.00102(3) -0.00149(3)
O1 0.0305(9) 0.0133(7) 0.0367(9) 0.0077(6) -0.0050(7) 0.0021(6)
O2 0.0186(7) 0.0257(8) 0.0187(7) -0.0003(6) -0.0053(6) -0.0106(6)
O3 0.0189(7) 0.0303(8) 0.0148(7) -0.0020(6) 0.0041(6) -0.0052(6)
N1 0.0092(7) 0.0088(7) 0.0112(7) -0.0001(5) -0.0013(5) -0.0006(5)
N2 0.0087(7) 0.0109(7) 0.0115(7) -0.0001(6) -0.0017(5) -0.0016(5)
N3 0.0088(7) 0.0094(7) 0.0116(7) -0.0008(6) -0.0013(5) -0.0009(5)
C1 0.0120(8) 0.0077(8) 0.0111(8) -0.0009(6) -0.0005(6) -0.0021(6)
C2 0.0137(9) 0.0082(8) 0.0138(8) -0.0016(6) 0.0020(7) -0.0013(6)
C3 0.0131(9) 0.0075(8) 0.0134(8) -0.0016(6) 0.0016(7) -0.0010(6)
C4 0.0106(8) 0.0072(8) 0.0144(8) -0.0003(6) 0.0001(6) -0.0002(6)
C5 0.0101(8) 0.0115(8) 0.0150(9) 0.0015(7) -0.0019(7) -0.0005(6)
C6 0.0103(8) 0.0110(8) 0.0120(8) 0.0018(6) -0.0033(6) -0.0020(6)
C7 0.0111(8) 0.0148(9) 0.0097(8) 0.0010(6) -0.0031(6) -0.0035(7)
C8 0.0137(9) 0.0146(9) 0.0095(8) 0.0010(6) -0.0030(6) -0.0038(7)
C9 0.0120(8) 0.0136(8) 0.0083(8) -0.0011(6) 0.0005(6) -0.0035(7)
C10 0.0111(8) 0.0129(9) 0.0120(8) -0.0030(7) 0.0015(6) -0.0023(7)
C11 0.0089(8) 0.0115(8) 0.0130(8) -0.0011(6) 0.0019(6) -0.0008(6)
C12 0.0086(8) 0.0117(8) 0.0160(9) -0.0006(7) 0.0016(6) -0.0005(6)
C13 0.0076(8) 0.0127(8) 0.0150(8) 0.0002(7) 0.0018(6) -0.0001(6)
C14 0.0070(8) 0.0113(8) 0.0135(8) 0.0012(6) -0.0012(6) -0.0014(6)
C15 0.0101(8) 0.0113(8) 0.0125(8) 0.0020(6) -0.0039(6) -0.0018(6)
C16 0.0117(8) 0.0111(8) 0.0115(8) -0.0004(6) -0.0019(6) -0.0026(6)
C17 0.0173(9) 0.0152(9) 0.0135(9) -0.0007(7) 0.0016(7) -0.0002(7)
C18 0.0100(8) 0.0120(9) 0.0180(9) -0.0008(7) 0.0024(7) -0.0008(7)
C19 0.0123(9) 0.0141(9) 0.0211(9) -0.0006(7) -0.0009(7) 0.0024(7)
C20 0.0136(9) 0.0125(9) 0.0289(11) -0.0001(8) 0.0005(8) -0.0002(7)
C21 0.0225(11) 0.0169(10) 0.0302(11) -0.0062(8) 0.0003(8) -0.0020(8)
C22 0.0110(9) 0.0198(9) 0.0157(9) 0.0002(7) -0.0039(7) -0.0032(7)
C23 0.0127(10) 0.0291(12) 0.0346(12) 0.0099(9) 0.0018(8) -0.0012(8)
C24 0.0177(9) 0.0174(9) 0.0165(9) -0.0035(7) -0.0049(7) -0.0033(7)
C25 0.0289(12) 0.0165(10) 0.0330(12) -0.0002(9) -0.0029(9) -0.0072(8)
C26 0.0136(9) 0.0111(9) 0.0192(9) -0.0032(7) 0.0010(7) 0.0004(7)
C27 0.0176(9) 0.0118(9) 0.0189(9) -0.0021(7) 0.0051(7) -0.0005(7)
C28 0.0248(11) 0.0127(9) 0.0226(10) -0.0038(8) 0.0075(8) -0.0003(8)
C29 0.0317(12) 0.0200(11) 0.0286(12) -0.0042(9) 0.0140(9) 0.0023(9)
C30 0.0133(9) 0.0147(9) 0.0189(9) 0.0000(7) -0.0025(7) 0.0034(7)
C31 0.0135(9) 0.0176(10) 0.0163(9) -0.0003(7) -0.0009(7) -0.0035(7)
C32 0.0144(9) 0.0128(9) 0.0127(8) 0.0004(7) 0.0011(7) -0.0016(7)
C33 0.0122(9) 0.0130(9) 0.0144(9) -0.0010(7) -0.0044(7) -0.0025(7)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C32 1.9236(19) . ?
Re1 C31 1.924(2) . ?
Re1 C33 1.9306(19) . ?
Re1 N3 2.1294(15) . ?
Re1 N1 2.1306(16) . ?
Re1 N2 2.1324(15) . ?
O1 C31 1.155(3) . ?
O2 C32 1.158(2) . ?
O3 C33 1.155(2) . ?
N1 C1 1.356(2) . ?
N1 C4 1.371(2) . ?
N2 C6 1.358(2) . ?
N2 C9 1.361(2) . ?
N3 C14 1.354(2) . ?
N3 C11 1.374(2) . ?
C1 C16 1.410(2) . ?
C1 C2 1.470(2) . ?
C2 C3 1.364(3) . ?
C2 C17 1.501(3) . ?
C3 C4 1.456(2) . ?
C3 C18 1.502(2) . ?
C4 C5 1.401(2) . ?
C5 C6 1.404(3) . ?
C5 H5 0.96(2) . ?
C6 C7 1.461(2) . ?
C7 C8 1.371(3) . ?
C7 C22 1.499(2) . ?
C8 C9 1.461(2) . ?
C8 C24 1.500(3) . ?
C9 C10 1.405(3) . ?
C10 C11 1.399(2) . ?
C10 H10 0.91(2) . ?
C11 C12 1.458(2) . ?
C12 C13 1.371(3) . ?
C12 C26 1.505(2) . ?
C13 C14 1.460(2) . ?
C13 C30 1.492(3) . ?
C14 C15 1.412(3) . ?
C15 C16 1.401(3) . ?
C15 H15 0.96(2) . ?
C16 H16 0.96(2) . ?
C17 H17A 0.9361 . ?
C17 H17B 0.9361 . ?
C17 H17C 0.9361 . ?
C18 C19 1.535(3) . ?
C18 H18A 0.9669 . ?
C18 H18B 0.9669 . ?
C19 C20 1.530(3) . ?
C19 H19A 0.9890 . ?
C19 H19B 0.9890 . ?
C20 C21 1.527(3) . ?
C20 H20A 0.9860 . ?
C20 H20B 0.9860 . ?
C21 H21A 1.0049 . ?
C21 H21B 1.0049 . ?
C21 H21C 1.0049 . ?
C22 C23 1.527(3) . ?
C22 H22A 0.9871 . ?
C22 H22B 0.9871 . ?
C23 H23A 0.9914 . ?
C23 H23B 0.9914 . ?
C23 H23C 0.9914 . ?
C24 C25 1.530(3) . ?
C24 H24A 0.9494 . ?
C24 H24B 0.9494 . ?
C25 H25A 1.0071 . ?
C25 H25B 1.0071 . ?
C25 H25C 1.0071 . ?
C26 C27 1.533(3) . ?
C26 H26A 0.9818 . ?
C26 H26B 0.9818 . ?
C27 C28 1.527(3) . ?
C27 H27A 0.9744 . ?
C27 H27B 0.9744 . ?
C28 C29 1.530(3) . ?
C28 H28A 0.9758 . ?
C28 H28B 0.9758 . ?
C29 H29A 0.9754 . ?
C29 H29B 0.9754 . ?
C29 H29C 0.9754 . ?
C30 H30A 0.9350 . ?
C30 H30B 0.9350 . ?
C30 H30C 0.9350 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C32 Re1 C31 89.35(8) . . ?
C32 Re1 C33 86.98(8) . . ?
C31 Re1 C33 86.52(8) . . ?
C32 Re1 N3 95.44(7) . . ?
C31 Re1 N3 173.94(7) . . ?
C33 Re1 N3 97.43(7) . . ?
C32 Re1 N1 97.31(7) . . ?
C31 Re1 N1 94.27(7) . . ?
C33 Re1 N1 175.64(6) . . ?
N3 Re1 N1 81.45(6) . . ?
C32 Re1 N2 170.96(7) . . ?
C31 Re1 N2 98.02(7) . . ?
C33 Re1 N2 98.65(7) . . ?
N3 Re1 N2 76.89(6) . . ?
N1 Re1 N2 77.00(6) . . ?
C1 N1 C4 107.69(15) . . ?
C1 N1 Re1 129.45(12) . . ?
C4 N1 Re1 120.70(12) . . ?
C6 N2 C9 107.41(15) . . ?
C6 N2 Re1 125.67(12) . . ?
C9 N2 Re1 126.89(12) . . ?
C14 N3 C11 108.05(15) . . ?
C14 N3 Re1 126.33(12) . . ?
C11 N3 Re1 123.14(12) . . ?
N1 C1 C16 124.63(16) . . ?
N1 C1 C2 109.32(15) . . ?
C16 C1 C2 125.75(16) . . ?
C3 C2 C1 106.52(16) . . ?
C3 C2 C17 128.22(17) . . ?
C1 C2 C17 125.03(16) . . ?
C2 C3 C4 106.75(16) . . ?
C2 C3 C18 130.13(17) . . ?
C4 C3 C18 122.99(16) . . ?
N1 C4 C5 122.90(16) . . ?
N1 C4 C3 109.35(15) . . ?
C5 C4 C3 125.75(17) . . ?
C4 C5 C6 122.44(17) . . ?
C4 C5 H5 117.6(14) . . ?
C6 C5 H5 117.6(14) . . ?
N2 C6 C5 120.90(16) . . ?
N2 C6 C7 109.69(16) . . ?
C5 C6 C7 126.90(17) . . ?
C8 C7 C6 106.28(16) . . ?
C8 C7 C22 128.74(17) . . ?
C6 C7 C22 124.73(17) . . ?
C7 C8 C9 106.36(16) . . ?
C7 C8 C24 128.62(17) . . ?
C9 C8 C24 124.74(17) . . ?
N2 C9 C10 121.50(16) . . ?
N2 C9 C8 109.58(16) . . ?
C10 C9 C8 126.51(17) . . ?
C11 C10 C9 122.46(17) . . ?
C11 C10 H10 116.7(15) . . ?
C9 C10 H10 119.1(15) . . ?
N3 C11 C10 122.54(16) . . ?
N3 C11 C12 109.03(15) . . ?
C10 C11 C12 127.01(17) . . ?
C13 C12 C11 106.40(16) . . ?
C13 C12 C26 127.50(17) . . ?
C11 C12 C26 125.93(16) . . ?
C12 C13 C14 106.92(16) . . ?
C12 C13 C30 126.87(17) . . ?
C14 C13 C30 126.12(16) . . ?
N3 C14 C15 125.29(16) . . ?
N3 C14 C13 109.14(15) . . ?
C15 C14 C13 124.63(16) . . ?
C16 C15 C14 132.11(17) . . ?
C16 C15 H15 115.4(14) . . ?
C14 C15 H15 111.6(14) . . ?
C15 C16 C1 132.06(17) . . ?
C15 C16 H16 112.9(14) . . ?
C1 C16 H16 114.4(14) . . ?
C2 C17 H17A 109.5 . . ?
C2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C3 C18 C19 113.83(15) . . ?
C3 C18 H18A 108.8 . . ?
C19 C18 H18A 108.8 . . ?
C3 C18 H18B 108.8 . . ?
C19 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C20 C19 C18 113.86(16) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C21 C20 C19 113.88(17) . . ?
C21 C20 H20A 108.8 . . ?
C19 C20 H20A 108.8 . . ?
C21 C20 H20B 108.8 . . ?
C19 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C22 C23 113.49(16) . . ?
C7 C22 H22A 108.9 . . ?
C23 C22 H22A 108.9 . . ?
C7 C22 H22B 108.9 . . ?
C23 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C8 C24 C25 113.34(17) . . ?
C8 C24 H24A 108.9 . . ?
C25 C24 H24A 108.9 . . ?
C8 C24 H24B 108.9 . . ?
C25 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C12 C26 C27 114.63(15) . . ?
C12 C26 H26A 108.6 . . ?
C27 C26 H26A 108.6 . . ?
C12 C26 H26B 108.6 . . ?
C27 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C28 C27 C26 111.17(16) . . ?
C28 C27 H27A 109.4 . . ?
C26 C27 H27A 109.4 . . ?
C28 C27 H27B 109.4 . . ?
C26 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C27 C28 C29 113.62(17) . . ?
C27 C28 H28A 108.8 . . ?
C29 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
C29 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C13 C30 H30A 109.5 . . ?
C13 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C13 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O1 C31 Re1 179.11(19) . . ?
O2 C32 Re1 178.28(17) . . ?
O3 C33 Re1 176.62(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C32 Re1 N1 C1 27.05(16) . . . . ?
C31 Re1 N1 C1 116.94(16) . . . . ?
N3 Re1 N1 C1 -67.39(15) . . . . ?
N2 Re1 N1 C1 -145.81(16) . . . . ?
C32 Re1 N1 C4 -134.04(14) . . . . ?
C31 Re1 N1 C4 -44.15(14) . . . . ?
N3 Re1 N1 C4 131.52(14) . . . . ?
N2 Re1 N1 C4 53.10(13) . . . . ?
C31 Re1 N2 C6 44.23(16) . . . . ?
C33 Re1 N2 C6 131.90(15) . . . . ?
N3 Re1 N2 C6 -132.43(15) . . . . ?
N1 Re1 N2 C6 -48.33(14) . . . . ?
C31 Re1 N2 C9 -137.74(15) . . . . ?
C33 Re1 N2 C9 -50.07(16) . . . . ?
N3 Re1 N2 C9 45.60(15) . . . . ?
N1 Re1 N2 C9 129.69(15) . . . . ?
C32 Re1 N3 C14 -25.53(16) . . . . ?
C33 Re1 N3 C14 -113.18(15) . . . . ?
N1 Re1 N3 C14 71.07(15) . . . . ?
N2 Re1 N3 C14 149.62(15) . . . . ?
C32 Re1 N3 C11 134.41(14) . . . . ?
C33 Re1 N3 C11 46.76(14) . . . . ?
N1 Re1 N3 C11 -128.99(14) . . . . ?
N2 Re1 N3 C11 -50.43(13) . . . . ?
C4 N1 C1 C16 -168.76(17) . . . . ?
Re1 N1 C1 C16 28.2(3) . . . . ?
C4 N1 C1 C2 5.20(19) . . . . ?
Re1 N1 C1 C2 -157.79(12) . . . . ?
N1 C1 C2 C3 -2.0(2) . . . . ?
C16 C1 C2 C3 171.91(17) . . . . ?
N1 C1 C2 C17 -176.78(16) . . . . ?
C16 C1 C2 C17 -2.9(3) . . . . ?
C1 C2 C3 C4 -1.90(19) . . . . ?
C17 C2 C3 C4 172.69(17) . . . . ?
C1 C2 C3 C18 -177.72(17) . . . . ?
C17 C2 C3 C18 -3.1(3) . . . . ?
C1 N1 C4 C5 158.31(17) . . . . ?
Re1 N1 C4 C5 -36.9(2) . . . . ?
C1 N1 C4 C3 -6.41(19) . . . . ?
Re1 N1 C4 C3 158.36(12) . . . . ?
C2 C3 C4 N1 5.2(2) . . . . ?
C18 C3 C4 N1 -178.62(16) . . . . ?
C2 C3 C4 C5 -159.00(18) . . . . ?
C18 C3 C4 C5 17.2(3) . . . . ?
N1 C4 C5 C6 -11.3(3) . . . . ?
C3 C4 C5 C6 150.84(18) . . . . ?
C9 N2 C6 C5 -154.97(17) . . . . ?
Re1 N2 C6 C5 23.4(2) . . . . ?
C9 N2 C6 C7 8.2(2) . . . . ?
Re1 N2 C6 C7 -173.41(11) . . . . ?
C4 C5 C6 N2 19.0(3) . . . . ?
C4 C5 C6 C7 -141.17(19) . . . . ?
N2 C6 C7 C8 -5.2(2) . . . . ?
C5 C6 C7 C8 156.73(18) . . . . ?
N2 C6 C7 C22 -179.85(16) . . . . ?
C5 C6 C7 C22 -17.9(3) . . . . ?
C6 C7 C8 C9 0.21(19) . . . . ?
C22 C7 C8 C9 174.55(17) . . . . ?
C6 C7 C8 C24 -173.81(18) . . . . ?
C22 C7 C8 C24 0.5(3) . . . . ?
C6 N2 C9 C10 155.36(17) . . . . ?
Re1 N2 C9 C10 -23.0(2) . . . . ?
C6 N2 C9 C8 -8.1(2) . . . . ?
Re1 N2 C9 C8 173.57(11) . . . . ?
C7 C8 C9 N2 4.8(2) . . . . ?
C24 C8 C9 N2 179.16(16) . . . . ?
C7 C8 C9 C10 -157.58(18) . . . . ?
C24 C8 C9 C10 16.7(3) . . . . ?
N2 C9 C10 C11 -17.0(3) . . . . ?
C8 C9 C10 C11 143.51(19) . . . . ?
C14 N3 C11 C10 -161.51(17) . . . . ?
Re1 N3 C11 C10 35.4(2) . . . . ?
C14 N3 C11 C12 5.76(19) . . . . ?
Re1 N3 C11 C12 -157.35(12) . . . . ?
C9 C10 C11 N3 10.2(3) . . . . ?
C9 C10 C11 C12 -154.66(18) . . . . ?
N3 C11 C12 C13 -2.2(2) . . . . ?
C10 C11 C12 C13 164.38(18) . . . . ?
N3 C11 C12 C26 -177.80(16) . . . . ?
C10 C11 C12 C26 -11.3(3) . . . . ?
C11 C12 C13 C14 -2.01(19) . . . . ?
C26 C12 C13 C14 173.53(17) . . . . ?
C11 C12 C13 C30 -178.80(17) . . . . ?
C26 C12 C13 C30 -3.3(3) . . . . ?
C11 N3 C14 C15 162.27(17) . . . . ?
Re1 N3 C14 C15 -35.3(2) . . . . ?
C11 N3 C14 C13 -7.01(19) . . . . ?
Re1 N3 C14 C13 155.40(12) . . . . ?
C12 C13 C14 N3 5.7(2) . . . . ?
C30 C13 C14 N3 -177.52(17) . . . . ?
C12 C13 C14 C15 -163.70(17) . . . . ?
C30 C13 C14 C15 13.1(3) . . . . ?
N3 C14 C15 C16 -19.1(3) . . . . ?
C13 C14 C15 C16 148.5(2) . . . . ?
C14 C15 C16 C1 3.0(4) . . . . ?
N1 C1 C16 C15 19.3(3) . . . . ?
C2 C1 C16 C15 -153.72(19) . . . . ?
C2 C3 C18 C19 -119.1(2) . . . . ?
C4 C3 C18 C19 65.7(2) . . . . ?
C3 C18 C19 C20 67.2(2) . . . . ?
C18 C19 C20 C21 63.9(2) . . . . ?
C8 C7 C22 C23 -87.5(2) . . . . ?
C6 C7 C22 C23 85.9(2) . . . . ?
C7 C8 C24 C25 93.3(2) . . . . ?
C9 C8 C24 C25 -79.8(2) . . . . ?
C13 C12 C26 C27 85.8(2) . . . . ?
C11 C12 C26 C27 -99.5(2) . . . . ?
C12 C26 C27 C28 -177.86(17) . . . . ?
C26 C27 C28 C29 177.31(18) . . . . ?